Method for making acylamides by synthesizing and acylating benzoxazines
a technology of acylamide and benzoxazines, which is applied in the field of making an acylamide of formula, can solve the problems of excessive waste generation
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example 1
[0034] o-nitrophenoxyacetone
[0035] The o-nitrophenoxyacetone is prepared by heating with agitation for five hours at about 65.degree. C. a mixture which consists of 421.6 g (3.006 moles) of o-nitrophenol, 297.8 g (3.09 moles) of chloroacetone, 37.2 g (96%, 0.3615 moles) of sodium bromide, 277.2 g (3.3 moles) of sodium bicarbonate, 21.8 g (0.0647 moles) of aqueous tributylmethylammonium chloride (TBMAC), and 829 g of toluene. There is then added 9.0 g (0.093 mole) of additional chloroacetone to the mixture which is further heated at 65.degree. C. for 2.5 hours (note, sample analysis indicated that the reaction was complete after 1.5 hours). There is then added, 570 g of water and the pH of the mixture is adjusted to 6.5-7 at 55.degree. C. to 60.degree. C. upon addition of 55 g of a 10% HCl solution. The phases are allowed to separate and the aqueous phase is removed.
[0036] There is added 600 g of a 5% NaCl solution to the organic phase and the resulting mixtures is vigorously agitate...
example 2
[0037] 3,4-dihydro-3-methyl-2H-1,4-benzoxazine (3-MBA)
[0038] A previously filtered mixture of 273.2 g (97%, 1.359 mole) of o-nitrophenoxyacetone, 178 g of toluene, and 44 g of isopropanol at 55-60.degree. C. is added over a three hour period to a Parr reactor under 200 psig of hydrogen pressure and containing an agitated mixture of 85.5 g of a water wet 5% platinum on carbon catalyst (24.1 g on dry basis, Engelhart), 168 g of toluene, and 42 g of isopropanol at 55-60.degree. C. During the addition, the hydrogen pressure and the temperature are maintained at 200 psig and 60.degree. C., respectively. At the end of the addition, the conditions of the reactor are maintained for an additional 60 minutes.
[0039] The pressure of the Parr reactor is initially relieved and then is opened. The cooling coils and agitator shaft are washed with toluene / isopropanol; the warm slurry is filtered under 7 to 15 psig pressure. The catalyst is filtered and washed with 140 g of toluene / isopropanol and 28...
example 3
[0040] (.+-.)-4-dichloroacetyl-3,4-dihydro-3-methyl-2H-1.4-benzoxazine (benoxacor)
[0041] a) o-Nitrophenoxyacetone (o-NPA)
[0042] The following materials are combined in a 1000 gallon vessel and heated at 65.degree. C. for 6-8 hours: 499.0 kg (1.000 mole equiv.) of o-Nitrophenol (o-NP, 99%, 3.551 kg-moles), 359.7 kg (1.05 mole equiv.) of chloroacetone (CA, 96%, 3.733 kg-moles), 45.4 kg (0.124 mole equiv.) of sodium bromide (0.441 kg-moles), 328.9 kg (1.102 mole equiv.) of sodium bicarbonate (3.915 kg-moles), 27.2 kg (0.023 mole equiv.) of aqueous tributylmethylammonium chloride (TBMAC, 70%, 0.081 kg-moles), and 989 kg of toluene. The reaction is checked for completion and a trim charge of chloroacetone is added if necessary. Then 682 kg of water are added at 60.degree. C. and the pH of the reaction mixture is adjusted to pH 6.5-7.0 at 55 to 60.degree. C. (about 66 kg of 10% HCl). The phases are separated and the heavier aqueous phase is removed. A 5-15% NaCl solution (725 kg) is added...
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